#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:38:12 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179254 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/74/4317419.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4317419
loop_
_publ_author_name
'Xian-He Bu'
'Wei Weng'
'Jian-Rong Li'
'Wei Chen'
'Ruo-Hua Zhang'
_publ_section_title
;
 Novel Five-Connected Lanthanide(III)-Bis(sulfinyl) Coordination Polymers
 Forming a Unique Two-Dimensional (3/4,5) Network
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              413
_journal_page_last               415
_journal_paper_doi               10.1021/ic010605b
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C23 H45 N3 Nd O5 S8'
_chemical_formula_weight         844.34
_chemical_name_systematic
;
   ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                97.639(4)
_cell_angle_beta                 96.240(5)
_cell_angle_gamma                97.378(5)
_cell_formula_units_Z            2
_cell_length_a                   9.105(2)
_cell_length_b                   12.472(3)
_cell_length_c                   17.450(4)
_cell_measurement_temperature    298(2)
_cell_volume                     1931.7(8)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0220
_diffrn_reflns_av_sigmaI/netI    0.0380
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            8149
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.19
_exptl_absorpt_coefficient_mu    1.809
_exptl_absorpt_correction_T_max  0.8398
_exptl_absorpt_correction_T_min  0.6130
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.452
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.970
_refine_diff_density_min         -1.485
_refine_diff_density_rms         0.233
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     356
_refine_ls_number_reflns         6790
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0539
_refine_ls_R_factor_gt           0.0411
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0829P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1103
_refine_ls_wR_factor_ref         0.1304
_reflns_number_gt                5673
_reflns_number_total             6790
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010605b_1.cif
_cod_data_source_block           complex1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        1931.9(8)
_cod_database_code               4317419
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Nd1 Nd 0.32921(3) 1.02380(2) 0.244067(14) 0.03734(12) Uani 1 1 d . . .
O1 O 0.5772(4) 1.1025(3) 0.3134(2) 0.0502(9) Uani 1 1 d . . .
O2 O 0.3608(4) 0.9120(3) 0.3489(2) 0.0520(10) Uani 1 1 d . . .
O3 O 0.0872(4) 0.9362(3) 0.2659(2) 0.0538(10) Uani 1 1 d . . .
O4 O 0.1963(4) 0.9376(4) 0.1150(2) 0.0586(10) Uani 1 1 d . . .
O5 O 0.4710(4) 1.1021(4) 0.1510(2) 0.0554(10) Uani 1 1 d . . .
S1 S 0.1717(3) 1.2434(3) 0.49477(14) 0.1345(13) Uani 1 1 d . . .
S2 S 0.6456(3) 0.7448(2) 0.11096(14) 0.1099(9) Uani 1 1 d . . .
S3 S -0.0087(3) 1.32027(18) 0.17746(15) 0.0895(6) Uani 1 1 d . . .
S4 S 0.71216(16) 1.15929(13) 0.28307(9) 0.0540(4) Uani 1 1 d . . .
S5 S 0.48906(15) 0.87762(12) 0.39730(9) 0.0493(3) Uani 1 1 d . . .
S6 S 0.01231(17) 0.91931(14) 0.33797(9) 0.0574(4) Uani 1 1 d . . .
S7 S 0.03348(19) 0.89448(18) 0.08890(10) 0.0752(5) Uani 1 1 d . . .
S8 S 0.44394(16) 1.14129(13) 0.07295(8) 0.0501(3) Uani 1 1 d . . .
N1 N 0.2748(6) 1.1429(5) 0.3640(3) 0.0665(15) Uani 1 1 d . . .
N2 N 0.4807(6) 0.8769(5) 0.1967(3) 0.0648(14) Uani 1 1 d . . .
N3 N 0.1807(7) 1.1674(5) 0.1984(3) 0.0699(15) Uani 1 1 d . . .
C1 C 0.2329(7) 1.1859(6) 0.4174(4) 0.0588(16) Uani 1 1 d . . .
C2 C 0.5488(7) 0.8202(5) 0.1625(3) 0.0548(15) Uani 1 1 d . . .
C3 C 0.1039(7) 1.2319(5) 0.1906(3) 0.0535(14) Uani 1 1 d . . .
C4 C 0.8411(8) 1.0595(8) 0.2775(5) 0.086(2) Uani 1 1 d . . .
H4A H 0.7968 0.9986 0.2378 0.103 Uiso 1 1 calc R . .
H4B H 0.9314 1.0929 0.2601 0.103 Uiso 1 1 calc R . .
C5 C 0.8027(9) 1.2567(7) 0.3637(5) 0.092(3) Uani 1 1 d . . .
H5A H 0.8193 1.2199 0.4088 0.110 Uiso 1 1 calc R . .
H5B H 0.8994 1.2874 0.3516 0.110 Uiso 1 1 calc R . .
C6 C 0.7163(13) 1.3456(7) 0.3831(7) 0.123(4) Uani 1 1 d . . .
H6A H 0.6206 1.3148 0.3963 0.148 Uiso 1 1 calc R . .
H6B H 0.6973 1.3809 0.3375 0.148 Uiso 1 1 calc R . .
C7 C 0.7931(17) 1.4312(8) 0.4504(7) 0.166(6) Uani 1 1 d . . .
H7A H 0.7323 1.4880 0.4591 0.249 Uiso 1 1 calc R . .
H7B H 0.8883 1.4620 0.4380 0.249 Uiso 1 1 calc R . .
H7C H 0.8074 1.3978 0.4966 0.249 Uiso 1 1 calc R . .
C8 C 0.4738(7) 0.9388(5) 0.4951(3) 0.0602(16) Uani 1 1 d . . .
H8A H 0.3708 0.9257 0.5052 0.072 Uiso 1 1 calc R . .
H8B H 0.5343 0.9061 0.5322 0.072 Uiso 1 1 calc R . .
C9 C 0.4270(8) 0.7387(5) 0.4070(4) 0.0704(19) Uani 1 1 d . . .
H9A H 0.4938 0.7161 0.4470 0.084 Uiso 1 1 calc R . .
H9B H 0.3280 0.7330 0.4232 0.084 Uiso 1 1 calc R . .
C10 C 0.4227(11) 0.6631(6) 0.3304(5) 0.094(3) Uani 1 1 d . . .
H10A H 0.3591 0.6874 0.2899 0.113 Uiso 1 1 calc R . .
H10B H 0.5224 0.6665 0.3153 0.113 Uiso 1 1 calc R . .
C11 C 0.3637(16) 0.5454(7) 0.3379(7) 0.151(5) Uani 1 1 d . . .
H11A H 0.3631 0.4994 0.2891 0.226 Uiso 1 1 calc R . .
H11B H 0.2640 0.5416 0.3514 0.226 Uiso 1 1 calc R . .
H11C H 0.4269 0.5211 0.3778 0.226 Uiso 1 1 calc R . .
C12 C -0.1160(9) 1.0157(7) 0.3498(5) 0.083(2) Uani 1 1 d . . .
H12A H -0.2051 0.9806 0.3672 0.099 Uiso 1 1 calc R . .
H12B H -0.0710 1.0758 0.3900 0.099 Uiso 1 1 calc R . .
C13 C -0.1097(8) 0.7937(5) 0.3096(5) 0.0705(19) Uani 1 1 d . . .
H13A H -0.1868 0.7890 0.3437 0.085 Uiso 1 1 calc R . .
H13B H -0.1575 0.7904 0.2567 0.085 Uiso 1 1 calc R . .
C14 C -0.0222(11) 0.6991(7) 0.3142(6) 0.102(3) Uani 1 1 d . . .
H14A H 0.0581 0.7060 0.2821 0.123 Uiso 1 1 calc R . .
H14B H 0.0218 0.7007 0.3676 0.123 Uiso 1 1 calc R . .
C15 C -0.1176(18) 0.5971(9) 0.2879(9) 0.185(7) Uani 1 1 d . . .
H15A H -0.0608 0.5379 0.2918 0.278 Uiso 1 1 calc R . .
H15B H -0.1590 0.5949 0.2346 0.278 Uiso 1 1 calc R . .
H15C H -0.1970 0.5904 0.3197 0.278 Uiso 1 1 calc R . .
C16 C -0.0073(9) 0.9407(7) -0.0042(5) 0.093(3) Uani 1 1 d . . .
H16A H 0.0607 0.9151 -0.0393 0.111 Uiso 1 1 calc R . .
H16B H -0.1082 0.9096 -0.0270 0.111 Uiso 1 1 calc R . .
C17 C 0.0324(13) 0.7547(9) 0.0512(7) 0.123(4) Uani 1 1 d . . .
H17A H -0.0692 0.7212 0.0317 0.148 Uiso 1 1 calc R . .
H17B H 0.0910 0.7499 0.0079 0.148 Uiso 1 1 calc R . .
C18 C 0.092(3) 0.6967(12) 0.1096(11) 0.241(10) Uani 1 1 d . . .
H18A H 0.1817 0.7420 0.1376 0.289 Uiso 1 1 calc R . .
H18B H 0.0206 0.6891 0.1464 0.289 Uiso 1 1 calc R . .
C19 C 0.128(2) 0.5978(16) 0.0870(13) 0.271(11) Uiso 1 1 d . . .
H19A H 0.1751 0.5713 0.1311 0.407 Uiso 1 1 calc R . .
H19B H 0.1947 0.6024 0.0484 0.407 Uiso 1 1 calc R . .
H19C H 0.0386 0.5486 0.0653 0.407 Uiso 1 1 calc R . .
C20 C 0.5428(7) 1.0568(5) 0.0103(3) 0.0581(15) Uani 1 1 d . . .
H20A H 0.5552 1.0885 -0.0368 0.070 Uiso 1 1 calc R . .
H20B H 0.6412 1.0537 0.0368 0.070 Uiso 1 1 calc R . .
C21 C 0.5717(9) 1.2670(6) 0.0834(4) 0.075(2) Uani 1 1 d . . .
H21A H 0.6701 1.2551 0.1048 0.091 Uiso 1 1 calc R . .
H21B H 0.5791 1.2888 0.0324 0.091 Uiso 1 1 calc R . .
C22 C 0.5208(14) 1.3584(7) 0.1364(6) 0.118(4) Uani 1 1 d . . .
H22A H 0.4499 1.3232 0.1662 0.142 Uiso 1 1 calc R . .
H22B H 0.6073 1.3914 0.1733 0.142 Uiso 1 1 calc R . .
C23 C 0.468(4) 1.4296(16) 0.1146(12) 0.52(3) Uani 1 1 d . . .
H23A H 0.4523 1.4803 0.1585 0.778 Uiso 1 1 calc R . .
H23B H 0.3736 1.4016 0.0836 0.778 Uiso 1 1 calc R . .
H23C H 0.5330 1.4663 0.0836 0.778 Uiso 1 1 calc R . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O5 Nd1 O3 145.30(13) . . ?
O5 Nd1 O2 139.58(13) . . ?
O3 Nd1 O2 70.41(13) . . ?
O5 Nd1 O1 72.84(13) . . ?
O3 Nd1 O1 141.63(13) . . ?
O2 Nd1 O1 76.99(13) . . ?
O5 Nd1 O4 75.07(14) . . ?
O3 Nd1 O4 73.05(13) . . ?
O2 Nd1 O4 119.48(14) . . ?
O1 Nd1 O4 143.16(13) . . ?
O5 Nd1 N1 120.55(17) . . ?
O3 Nd1 N1 77.13(17) . . ?
O2 Nd1 N1 75.74(17) . . ?
O1 Nd1 N1 75.68(16) . . ?
O4 Nd1 N1 137.87(16) . . ?
O5 Nd1 N2 75.43(17) . . ?
O3 Nd1 N2 108.59(17) . . ?
O2 Nd1 N2 73.28(16) . . ?
O1 Nd1 N2 79.87(16) . . ?
O4 Nd1 N2 74.95(16) . . ?
N1 Nd1 N2 144.00(18) . . ?
O5 Nd1 N3 75.50(16) . . ?
O3 Nd1 N3 83.52(17) . . ?
O2 Nd1 N3 142.39(16) . . ?
O1 Nd1 N3 112.81(17) . . ?
O4 Nd1 N3 75.38(17) . . ?
N1 Nd1 N3 72.26(19) . . ?
N2 Nd1 N3 142.71(18) . . ?
S4 O1 Nd1 129.8(2) . . ?
S5 O2 Nd1 136.9(2) . . ?
S6 O3 Nd1 134.4(2) . . ?
S7 O4 Nd1 131.2(2) . . ?
S8 O5 Nd1 138.9(2) . . ?
O1 S4 C5 104.4(3) . . ?
O1 S4 C4 104.8(3) . . ?
C5 S4 C4 101.7(4) . . ?
O2 S5 C9 104.8(3) . . ?
O2 S5 C8 103.5(3) . . ?
C9 S5 C8 98.0(3) . . ?
O3 S6 C13 104.1(3) . . ?
O3 S6 C12 108.4(3) . . ?
C13 S6 C12 102.1(4) . . ?
O4 S7 C17 104.3(4) . . ?
O4 S7 C16 104.9(3) . . ?
C17 S7 C16 96.6(5) . . ?
O5 S8 C21 104.0(3) . . ?
O5 S8 C20 103.6(3) . . ?
C21 S8 C20 98.0(3) . . ?
C1 N1 Nd1 170.4(6) . . ?
C2 N2 Nd1 166.6(5) . . ?
C3 N3 Nd1 167.4(5) . . ?
N1 C1 S1 178.0(7) . . ?
N2 C2 S2 177.0(6) . . ?
N3 C3 S3 178.1(7) . . ?
C12 C4 S4 116.7(6) 1_655 . ?
C6 C5 S4 112.7(6) . . ?
C5 C6 C7 113.7(10) . . ?
C8 C8 S5 109.7(5) 2_676 . ?
C10 C9 S5 111.2(5) . . ?
C11 C10 C9 111.1(8) . . ?
C4 C12 S6 113.0(5) 1_455 . ?
C14 C13 S6 109.7(6) . . ?
C15 C14 C13 110.5(10) . . ?
C16 C16 S7 111.4(7) 2_575 . ?
C18 C17 S7 111.2(10) . . ?
C19 C18 C17 118.2(19) . . ?
C20 C20 S8 110.0(5) 2_675 . ?
C22 C21 S8 111.6(6) . . ?
C23 C22 C21 124.2(13) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Nd1 O5 2.410(4) . ?
Nd1 O3 2.423(4) . ?
Nd1 O2 2.458(4) . ?
Nd1 O1 2.459(4) . ?
Nd1 O4 2.475(4) . ?
Nd1 N1 2.534(5) . ?
Nd1 N2 2.538(5) . ?
Nd1 N3 2.538(5) . ?
O1 S4 1.519(4) . ?
O2 S5 1.507(4) . ?
O3 S6 1.520(4) . ?
O4 S7 1.509(4) . ?
O5 S8 1.514(4) . ?
S1 C1 1.630(6) . ?
S2 C2 1.622(7) . ?
S3 C3 1.621(6) . ?
S4 C5 1.781(8) . ?
S4 C4 1.818(8) . ?
S5 C9 1.788(7) . ?
S5 C8 1.802(6) . ?
S6 C13 1.778(7) . ?
S6 C12 1.789(8) . ?
S7 C17 1.778(11) . ?
S7 C16 1.812(8) . ?
S8 C21 1.804(7) . ?
S8 C20 1.807(6) . ?
N1 C1 1.139(8) . ?
N2 C2 1.149(7) . ?
N3 C3 1.142(7) . ?
C4 C12 1.474(10) 1_655 ?
C5 C6 1.465(12) . ?
C6 C7 1.518(14) . ?
C8 C8 1.520(12) 2_676 ?
C9 C10 1.524(11) . ?
C10 C11 1.524(12) . ?
C12 C4 1.474(10) 1_455 ?
C13 C14 1.512(10) . ?
C14 C15 1.434(14) . ?
C16 C16 1.453(16) 2_575 ?
C17 C18 1.427(19) . ?
C18 C19 1.33(2) . ?
C20 C20 1.506(12) 2_675 ?
C21 C22 1.524(12) . ?
C22 C23 1.151(19) . ?
